CN113929457A - Zirconium oxide powder and preparation method thereof - Google Patents
Zirconium oxide powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims description 22
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002244 precipitate Substances 0.000 claims abstract description 50
- 239000000084 colloidal system Substances 0.000 claims abstract description 34
- 239000011259 mixed solution Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 229910006251 ZrOCl2.8H2O Inorganic materials 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000003828 vacuum filtration Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000012716 precipitator Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 9
- 238000001556 precipitation Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 8
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000004570 mortar (masonry) Substances 0.000 abstract 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 7
- 239000000292 calcium oxide Substances 0.000 description 7
- 239000011575 calcium Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- 230000009466 transformation Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 238000000975 co-precipitation Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Inorganic materials [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004643 material aging Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 210000003781 tooth socket Anatomy 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/486—Fine ceramics
- C04B35/488—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The invention relates to zirconia powder and a preparation method thereof, belonging to the technical field of nano ceramic material preparation. The invention comprises the following steps: (1) respectively configuring ZrOCl2﹒8H2O and Ca (NO)3)2An aqueous solution; (2) according to ZrO2And Y2O3Preparing a mixed solution according to the molar ratio, and adding a dispersing agent; (3) adding the solution to a precipitant solution; (4) continuously generating colloid in the dropwise adding process, measuring the pH value of the mixed solution, converting the colloid into precipitate when the pH value is 7-8, and completely converting into precipitate when the pH value reaches 9-10; (5) standing the precipitate solution, vacuum filtering, cleaning, and drying the cleaned precipitate; (6) grinding the precipitate in a mortar, and calcining. The invention has scientific and reasonable design, simple and easy operation and low cost, and the obtained powder has high strength, uniform particles and better performanceGood sintering stability.
Description
Technical Field
The invention relates to zirconia powder and a preparation method thereof, belonging to the technical field of nano ceramic material preparation.
Background
The nanometer ceramic material has superplasticity and special properties of electricity, light, heat, magnetism and the like, so that the nanometer ceramic material becomes a research hotspot in the field of material science, nanometer zirconia is an important ceramic material and has the stable characteristics of high strength, corrosion resistance, heat resistance, low heat conductivity coefficient, strong oxidation resistance and the like, so that the nanometer zirconia is widely concerned by the material field and widely applied to optical fiber ferrules, optical fiber sleeves, teeth, tooth sockets, watchcases, cutting tools and the like, the zirconia powder is used as a basic industry of material supply, the requirements of various industries on the nanometer ceramic material are in an outbreak trend along with the continuous rise of high domestic requirements in the coming years, and domestic leading enterprises can also take the opportunity to develop the domestic market by the aid of the nanometer zirconia powder, and domestic challenges are met to deepen the autonomous research and development capability.
At present, the most applied methods for preparing zirconia powder are a sol-gel method, a hydrolysis method and a coprecipitation method, but in the prior art, the powder agglomeration phenomenon occurs in the powder preparation process, so that the later-stage forming processing and sintering of the powder are directly influenced, and the performance of zirconia ceramic is deteriorated.
Disclosure of Invention
The invention aims to provide a preparation method of zirconia powder, which has scientific and reasonable design, simple and easy operation and low cost, and the obtained powder has high strength, uniform particles and better sintering stability.
The preparation method of the zirconium oxide powder comprises the following steps:
(1) respectively preparing ZrOCl with the concentration of 0.05mol/L to 0.5mol/L2﹒8H2O and Ca (NO)3)2An aqueous solution;
(2) according to ZrO2And CaO in a molar ratio of 93-98: 7-2, preparing a mixed solution, and adding a dispersing agent;
(3) slowly adding the solution obtained in the step (2) into an excessive precipitator solution;
(4) continuously generating zirconium hydroxide colloid in the process of dropwise adding, gradually increasing flocculent colloid along with the continuous dropwise adding, measuring the pH value of the mixed solution by using a pH tester, converting the colloid into precipitate when the pH value is 7-8, and completely converting the flocculent colloid into precipitate when the pH value reaches 9-10;
(5) standing the precipitate solution for 18-36 h, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate with distilled water and ethanol for several times, and drying the washed precipitate in a constant-temperature air-blast drying oven at 70-85 ℃ for 12-24 h;
(6) putting the dried precipitate into a bowl body, grinding for 1-3 h, and calcining for 2-4 h at 700-1000 ℃ to obtain the zirconium oxide powder.
Preferably, the dispersant is one or more of polyethylene glycol (PEG2000), glycerol or acrylate.
Preferably, the addition amount of the dispersing agent is 0.01 to 0.2 percent of the mass of the mixed solution.
Preferably, the precipitant is aqueous ammonia.
Preferably, the concentration of the precipitant is 15g/L to 50 g/L.
The method for preparing the zirconia powder reduces the particle size of the powder by reducing the crystal particle size, and has the defect of causing mass agglomeration of the powder; at present, the most common stabilizer in the preparation process of the zirconia powder is yttria, and calcium oxide is selected as the stabilizer, so that the source is wider, the cost is lower, and the effect is better; ammonia water is selected as a precipitator, a uniform reaction system is formed under the action of strong alkali, and high polymer precipitate can be formed, so that smaller particle size is obtained during later calcination; the invention uses the organic additive-strong alkali coprecipitation method to ensure the consistency of the surrounding environment of the zirconium oxychloride during the reaction, and the tetragonal phase nano zirconium oxide powder which is stable at room temperature is obtained.
The invention has the following beneficial effects:
(1) the nano zirconia powder prepared by the method has small particle size (40-60 nm) and large specific surface area (8-9 m)2The main crystal phase is a tetragonal phase, and the aging stability is strong;
(2) the method adopts a coprecipitation method to prepare the zirconium oxide powder, has simple operation and lower cost, and the powder is not easy to agglomerate in the treatment engineering and is easy for industrial production.
Drawings
FIG. 1 is a schematic view showing a state of a zirconia powder fired according to the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
Example 1
A preparation method of zirconia powder comprises the following steps:
1) respectively preparing 0.1mol/L ZrOCl2﹒8H2O and Ca (NO)3)2An aqueous solution;
2) according to ZrO2And CaO in a molar ratio of 94: 6 preparing a mixed solution, and adding 0.01 percent of PEG 2000;
3) slowly adding the mixed solution into an excessive ammonia water solution with the concentration of 15 g/L;
4) constantly produce the zirconium hydroxide colloid at the in-process of dropwise add, along with constantly dropwise add, the flocculent colloid increases gradually, surveys the pH value of its mixed solution with the pH tester, and when pH value was 7 ~ 8, the colloid can be to deposiing the transformation, and when pH reachd 9 ~ 10, the flocculent colloid was changed into the sediment completely.
5) Standing the precipitate solution for 18h, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate for 2 times by using distilled water and ethanol, and drying the washed precipitate in a constant-temperature air-blast drying oven at the temperature of 75 ℃ for 12 h;
6) and putting the dried precipitate into a bowl body, grinding for 1h, and calcining for 2h at 800 ℃ to obtain the zirconium oxide powder.
Example 2
A preparation method of zirconia powder comprises the following steps:
1) respectively preparing 0.2mol/L ZrOCl2﹒8H2O and Ca (NO)3)2An aqueous solution;
2) according to ZrO2And CaO in a molar ratio of 96: 4 preparing a mixed solution, and adding 0.01% of glycerol;
3) slowly adding the mixed solution into an excessive ammonia water solution with the concentration of 20 g/L;
4) constantly produce the zirconium hydroxide colloid at the in-process of dropwise add, along with constantly dropwise add, the flocculent colloid increases gradually, surveys the pH value of its mixed solution with the pH tester, and when pH value was 7 ~ 8, the colloid can be to deposiing the transformation, and when pH reachd 9 ~ 10, the flocculent colloid was changed into the sediment completely.
5) Standing the precipitate solution for 18h, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate for 2 times by using distilled water and ethanol, and drying the washed precipitate in a constant-temperature air-blast drying oven at the temperature of 75 ℃ for 12 h;
6) and putting the dried precipitate into a bowl body, grinding for 1h, and calcining for 2h at 900 ℃ to obtain the zirconium oxide powder.
Example 3
A preparation method of zirconia powder comprises the following steps:
1) respectively preparing 0.3mol/L of ZrOCl2﹒8H2O and Ca (NO)3)2An aqueous solution;
2) according to ZrO2And CaO in a molar ratio of 98: 2 preparing a mixed solution, and adding 0.01% of glycerol;
3) slowly adding the mixed solution into an excessive ammonia water solution with the concentration of 25 g/L;
4) constantly produce the zirconium hydroxide colloid at the in-process of dropwise add, along with constantly dropwise add, flocculent colloid increases gradually, surveys its mixed solution's pH value with the pH tester, and when pH value was 7, the colloid can be to deposiing the transformation, and when pH reachd 9 ~ 10, flocculent colloid was transformed into the sediment completely.
5) Standing the precipitate solution for 18h, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate for 2 times by using distilled water and ethanol, and drying the washed precipitate in a constant-temperature air-blast drying oven at 85 ℃ for 12 h;
6) and putting the dried precipitate into a bowl body, grinding for 1h, and calcining for 2h at 950 ℃ to obtain the zirconium oxide powder.
Example 4
A preparation method of zirconia powder comprises the following steps:
1) respectively preparing 0.4mol/L of ZrOCl2﹒8H2O and Ca (NO)3)2An aqueous solution;
2) according to ZrO2And CaO in a molar ratio of 95: 5 preparing a mixed solution, and adding 0.02% of acrylate;
3) slowly adding the mixed solution into an excessive ammonia water solution with the concentration of 15 g/L;
4) constantly produce the zirconium hydroxide colloid at the in-process of dropwise add, along with constantly dropwise add, flocculent colloid increases gradually, surveys its mixed solution's pH value with the pH tester, and when pH value was 7, the colloid can be to deposiing the transformation, and when pH reachd 9 ~ 10, flocculent colloid was transformed into the sediment completely.
5) Standing the precipitate solution for 18h, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate for 2 times by using distilled water and ethanol, and drying the washed precipitate in a constant-temperature air-blast drying oven at the temperature of 80 ℃ for 12 h;
6) and putting the dried precipitate into a bowl body, grinding for 1h, and calcining for 2h at 1000 ℃ to obtain the zirconium oxide powder.
Comparative example 1
A preparation method of zirconia powder comprises the following steps:
1) respectively preparing 0.1mol/L ZrOCl2﹒8H2O and Ca (NO)3)2An aqueous solution;
2) according to ZrO2And CaO in a molar ratio of 94: 6 preparing a mixed solution, and adding 0.01 percent of PEG 2000;
3) slowly adding the mixed solution into excess KOH solution with the concentration of 15 g/L;
4) constantly produce the zirconium hydroxide colloid at the in-process of dropwise add, along with constantly dropwise add, the flocculent colloid increases gradually, surveys the pH value of its mixed solution with the pH tester, and when pH value was 7 ~ 8, the colloid can be to deposiing the transformation, and when pH reachd 9 ~ 10, the flocculent colloid was changed into the sediment completely.
5) Standing the precipitate solution for 18h, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate for 2 times by using distilled water and ethanol, and drying the washed precipitate in a constant-temperature air-blast drying oven at the temperature of 75 ℃ for 12 h;
6) and putting the dried precipitate into a bowl body, grinding for 1h, and calcining for 2h at 800 ℃ to obtain the zirconium oxide powder.
Comparative example 2
A preparation method of zirconia powder comprises the following steps:
1) respectively preparing 0.2mol/L ZrOCl2﹒8H2O and CsNO3An aqueous solution;
2) according to ZrO2And Cs2The molar ratio of O is 96: 4 preparing a mixed solution, and adding 0.01% of glycerol;
3) slowly adding the mixed solution into an excessive ammonia water solution with the concentration of 20 g/L;
4) constantly produce the zirconium hydroxide colloid at the in-process of dropwise add, along with constantly dropwise add, the flocculent colloid increases gradually, surveys the pH value of its mixed solution with the pH tester, and when pH value was 7 ~ 8, the colloid can be to deposiing the transformation, and when pH reachd 9 ~ 10, the flocculent colloid was changed into the sediment completely.
5) Standing the precipitate solution for 18h, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate for 2 times by using distilled water and ethanol, and drying the washed precipitate in a constant-temperature air-blast drying oven at the temperature of 75 ℃ for 12 h;
6) and putting the dried precipitate into a bowl body, grinding for 1h, and calcining for 2h at 900 ℃ to obtain the zirconium oxide powder.
The performance tests were performed on the zirconia powders prepared in examples 1 to 4 and the zirconia powders prepared in comparative examples 1 to 2:
the particle size detection method is a GB 6288-86 granular molecular sieve particle size determination method;
the strength detection method is a GB/T232-;
the specific surface area detection method is GB/T8074-;
the crystal phase detection method is a GB/T1555-1997 semiconductor single crystal orientation detection method;
the aging stability detection method is GB/T15750-1995 piezoceramic material aging performance test protocol.
TABLE 1 physical Properties of zirconia powder
Claims (10)
1. A preparation method of zirconia powder is characterized by comprising the following steps: the method comprises the following steps:
(1) respectively configuring ZrOCl2﹒8H2O and Ca (NO)3)2An aqueous solution;
(2) according to ZrO2Preparing a mixed solution according to the mol ratio of CaO and adding a dispersing agent;
(3) adding the solution obtained in the step (2) into an excessive precipitator solution;
(4) continuously generating zirconium hydroxide colloid in the process of dropwise adding, gradually increasing flocculent colloid along with the continuous dropwise adding, measuring the pH value of the mixed solution by using a pH tester, converting the colloid into precipitate when the pH value is 7-8, and completely converting the flocculent colloid into precipitate when the pH value reaches 9-10;
(5) standing the precipitate solution, carrying out vacuum filtration on the precipitate, then sequentially washing the precipitate with distilled water and ethanol, and drying the washed precipitate in a constant-temperature air-blast drying oven;
(6) and (4) placing the dried precipitate into a bowl grinding body for grinding, and then calcining to obtain the zirconium oxide powder.
2. The method for producing a zirconium oxide powder according to claim 1, characterized in that: in step (1), ZrOCl2﹒8H2O and Ca (NO)3)2The concentration of the aqueous solution is 0.05 mol/L-0.5 mol/L.
3. The method for producing a zirconium oxide powder according to claim 1, characterized in that: in the step (2), ZrO2And CaO in a molar ratio of 93-98: 7 to 2.
4. The method for producing a zirconium oxide powder according to claim 1, characterized in that: the dispersant is one or more of polyethylene glycol, glycerol or acrylate.
5. The method for producing a zirconium oxide powder according to claim 1, characterized in that: the addition amount of the dispersant is 0.01-0.2% of the mass of the mixed solution.
6. The method for producing a zirconium oxide powder according to claim 1, characterized in that: the precipitant is ammonia water.
7. The method for producing a zirconium oxide powder according to claim 1, characterized in that: the concentration of the precipitant is 15 g/L-50 g/L.
8. The method for producing a zirconium oxide powder according to claim 1, characterized in that: in the step (5), standing the precipitation solution for 18-36 h; drying for 12-24 h in a constant temperature blast drying oven at 70-85 ℃.
9. The method for producing a zirconium oxide powder according to claim 1, characterized in that: in the step (6), grinding is carried out for 1 h-3 h, and then calcination is carried out for 2 h-4 h at 700 ℃ -1000 ℃.
10. A zirconia powder characterized by: the method for producing a zirconium oxide powder according to any one of claims 1 to 9.
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